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How cold should a freezer be for naptha freeze precip? Options
 
jayjay001
#1 Posted : 2/26/2012 7:28:37 AM
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VM+P Naptha.

I know the pulls are working, as evaporation succeeds in getting me a decent amount of crystalization, but other than that.... I get some powder that just floats around distributed fairly evenly across the solvent, and doesn't work well filtering through a coffee filter.

So far, I've only managed to make any decent crystals is with bestine, and that's been hit or miss (mostly miss so far).

I'm just wondering if I could get some general ideas on how cold is cold enough? How much does this depend on the quantity of solvent and the concentration of DMT? It's annoying to evap everything so much, but I'm thinking I'll need a better freezer (not going to happen) if I want to avoid it.

Just fyi, using .5ml of naptha per 1g mhrb on heated pulls up to about 60C.
 

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Visty
#2 Posted : 2/26/2012 9:56:19 AM

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I think I read that -15 C should do it. But crystallization seems to be about leaving the container undisturbed too and that longer freezing times, that is, longer than the 24 hours that are often mentioned could help too.

 
jayjay001
#3 Posted : 2/26/2012 2:32:20 PM
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I'm going to try leaving my latest container for 48 hours, untouched, but I've already taken it out to check on the crystal formation... I'm way too impatient and curious. Must. Have. Patience.
 
seeohhdee
#4 Posted : 2/27/2012 6:22:18 AM

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this isnt gospel, just based on my limited knowledge of physics and chemistry...

there is no set temperature OR set amount of time for freeze precipitation, it is all a function of volume, temperature and pressure. pressure is constant so less volume (of solvent) means more dmt will fall out when the saturation point is reached (this varies based on dmt content and volume of solvent)

it is also sort of pointless to leave it in the freezer for any more time than it takes the solvent to reach the temperature of the freezer (if your freezer is set at -20C, then you are not going to get any more crystals after your solvent reaches that temperature (48 hours is WAY too long unless you are freezing gallons of solvent). i find that a few hours is sufficient to bring the solvent down to the temperature of my freezer

for example, you can have dmt-rich solvent at room temperature and it will begin to precipitate the second you decrease the temperature by even a degree

for maximum effect, though you just want to have as LITTLE solvent as possible and make it as COLD as possible. no hard rules...

but you are right about patience. that is key. i think the best thing to do is to let the solvent COMPLETELY evaporate and then take the stuff and re-crystalize (there are many re-x teks on this site)... the idea behind re-crystalization is that you put ALL of your rough product in as LITTLE solvent as possible at a high temp so when you put it in the freezer, most of your dmt falls out SUPER fast and SUPER pure

this takes a lot of time, though. its like the old adage says, anything worth having is worth waiting for.

hope this helps
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deeplake
#5 Posted : 2/27/2012 10:09:31 PM

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seeohhdee wrote:
it is also sort of pointless to leave it in the freezer for any more time than it takes the solvent to reach the temperature of the freezer (if your freezer is set at -20C, then you are not going to get any more crystals after your solvent reaches that temperature (48 hours is WAY too long unless you are freezing gallons of solvent). i find that a few hours is sufficient to bring the solvent down to the temperature of my freezer



I freeze precip just long enough ^ like he said, and I reuse the solvent. I don't like the dust, oder, ect. of evaporating either. Although last time I did evap my solvent cause I don't plan on extracting again for a long time, and was suprised at how much was in their! About .75 gms.
And the bestine (heptane) works great for rex agreed. But do you use it to pull the freebase too? Instead of naptha? Hmmm.
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alert
#6 Posted : 2/27/2012 10:22:17 PM
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If your freezer will freeze ice cream hard it is cold enough. You should reduce your solvent via evaporation until it gets cloudy at room temperature, then put it in the freezer. You want it to be super saturated with DMT so it will all crash out. If your solvent isn't saturated enough little or nothing will come out.
 
jayjay001
#7 Posted : 2/28/2012 1:57:47 PM
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Yeah, my solvent hasn't been getting cloudy at all at room temperature.

The only cloudy solvent I've seen so far is with heated Bestine dropped into an evapped solution for crystalization.


I've done heated heptane and naptha pulls from my spice but only got yellowish liquid at first.

I'm starting to think that my bark has a low concentration of DMT, because I'm getting extremely little out of it, no matter how how much I pull with or what temperature I pull at.
 
tony
#8 Posted : 2/28/2012 2:19:26 PM

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jayjay001 wrote:
Yeah, my solvent hasn't been getting cloudy at all at room temperature.


The cloudiness is not to do with temperature, it is indicative of how saturated the solvent is. So when alert said reduce it til it is cloudy at room temp, he/she meant leave it sitting evaporating at room temp until it gets cloudy. If it's not cloudy then a freeze precip isn't going to crash out most of what is in the solvent. This was an issue I had with my first extraction, the tek I followed used too much naphtha and I ended up having to evap it to about a third of the amount before it went cloudy.
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jayjay001
#9 Posted : 2/28/2012 2:27:33 PM
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Oh I understand that.

I was making the point that even if I used a relatively small amount of heptane or naptha (.5ml per g of bark) and heated the materials while pulling, and even did a reasonable number of agitation/separation cycles, there was never a decent milky color, and never a decent amount of dmt pulled.
 
Vodsel
#10 Posted : 2/28/2012 2:31:00 PM

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Imo, either increase the pH of the mix by basifying more, or try with a different MHRB supplier. That happened to me in my first STB attempt, I finally gave up (although I should have tried to add more NaOH) and the next time, with different MHRB and dry lime tek, results were excellent. Solvent was cloudy (no previous evap) within 20 minutes of being placed in a plain old freezer.
 
Lysergik
#11 Posted : 2/28/2012 4:09:33 PM

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If there is this symbol [โˆ—[โˆ—โˆ—โˆ—] on your freezer, I think it's cold enough (it worked for me @ 0.5ml of naphta CAS :
64742-49-0).

The few freezers I've checked all had this symbol. If you can, put it on his max power.
 
 
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